CN107267815A - A kind of aluminum gallium alloy and preparation method thereof, aluminium hydrate nano rod and preparation method thereof - Google Patents
A kind of aluminum gallium alloy and preparation method thereof, aluminium hydrate nano rod and preparation method thereof Download PDFInfo
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- CN107267815A CN107267815A CN201710447786.5A CN201710447786A CN107267815A CN 107267815 A CN107267815 A CN 107267815A CN 201710447786 A CN201710447786 A CN 201710447786A CN 107267815 A CN107267815 A CN 107267815A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
- C01F7/428—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation in an aqueous solution
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of aluminum gallium alloy and preparation method thereof, aluminium hydrate nano rod and preparation method thereof, belong to nano-aluminum hydroxide preparing technical field.Ga, In, Sn mass percent sum are 5~15% in aluminum gallium alloy of the present invention, and described Ga, In, Sn mass ratio are 65:22:13, surplus is Al and inevitable impurity.Aluminum gallium alloy of the present invention, available for preparing aluminium hydrate nano rod, low melting point phase (the Ga In Sn eutectics that Ga, In, Sn are formed, GIS) it is covered in aluminium grain surface, not only destroy the integrality of alumite, diffusion admittance also is provided to participate in the aluminium of reaction, can significantly shorten the aluminum-water reaction time, reaction efficiency is improved.
Description
Technical field
The present invention relates to a kind of aluminum gallium alloy and preparation method thereof, aluminium hydrate nano rod and preparation method thereof, belong to and receive
Rice aluminium hydroxide preparing technical field.
Background technology
Industrially, the hydroxide of aluminium has very important purposes.Aluminium hydroxide is that consumption is maximum and most widely used
Inorganic fire-retarded additive, be also the basic material of aluminum electrolysis industry aluminum oxide, it may also be used for prepare glass, ceramics, lubricant
Deng.Compared with conventional aluminium hydroxide, nano-aluminum hydroxide particle size is small, specific surface area big, with more excellent performance.With
Brand-new material the reach of science and various countries' environmental protection, gradually perfect and increasingly strict, the nano-aluminum hydroxide demand of flame retardant regulation
Amount will be increasing, with wide market prospects.The preparation method of nano-aluminum hydroxide has much now, mainly there is carbonization
Method, the precipitation method, hydro-thermal method, sol-gel process, micro emulsion method etc., but above-mentioned preparation method often exist complex technical process, into
The shortcomings of this height, environmental pollution, and react to prepare that nano-aluminum hydroxide its technical process is simple, cost is relatively low using aluminium and water
And reaction product is environmentally safe.But because aluminium surface is easily aoxidized and forms one layer of dense oxidation film, therefore in room temperature very
Into boiling water, aluminium is difficult to be reacted with water.Therefore how to destroy and prevent the oxide-film of aluminium surface formation just to turn into aluminum-water reaction system
Key issue in standby nano-aluminum hydroxide technology.
Because the oxide of aluminium can constantly dissolve in alkali environment, aluminum-water reaction can be promoted, but aqueous slkali has necessarily
Corrosivity, aluminum-water reaction needs to carry out in special equipment, therefore promotes aluminum-water reaction to prepare a nanometer hydrogen using aqueous slkali
There is limitation in the method for aluminum oxide.The oxide-film of aluminium surface can be destroyed using the method processing aluminium powder of mechanical ball mill and promote aluminium
Water reacts, and the aluminium powder after ball-milling treatment can react with neutral water, so this hydrogen producing technology is comparatively safe, but use this method
Ball-milling Time needed for preparing aluminium powder is long, generally more than more than ten hour, and the aluminium powder storage after ball milling is more difficult, need to be in inertia
Preserved in gaseous environment, in addition, powder, which has serious problem of aging, i.e. powder, places a period of time (once week) loss one
Point reactivity, so as to reduce aluminum-water reaction speed and aluminium hydroxide conversion ratio, while to prepare nano-aluminum hydroxide anti-for this method
Answer temperature also higher.
Application publication number discloses a kind of high pure and ultra-fine nano-aluminum hydroxide for CN106277003A Chinese invention patent
Preparation method, mixed using activated aluminum powder with water, at the same add aluminum oxide nano-aluminum hydroxide is prepared as crystal seed, react
Temperature is 85~95 DEG C, and the reaction time is 24~48h, and reaction temperature needed for preparing nano-aluminum hydroxide using this method is high, anti-
Long and low production efficiency between seasonable.
The content of the invention
It is an object of the invention to provide a kind of aluminum gallium alloy, aluminium hydrate nano rod is prepared using the aluminum gallium alloy, is solved
Determine the low technical problem of temperature height, reaction time length, efficiency needed for preparing nano-aluminum hydroxide in the prior art.
Second purpose of the invention is to provide a kind of preparation method of above-mentioned aluminum gallium alloy.
3rd purpose of the invention is to provide a kind of method for preparing aluminium hydrate nano rod using above-mentioned aluminum gallium alloy.
4th purpose of the invention is to provide a kind of aluminium hydrate nano rod.
To achieve the above object, the technical scheme is that：
Ga, In, Sn mass percent sum are 5~15% in a kind of aluminum gallium alloy, the aluminum gallium alloy, the Ga,
In, Sn mass ratio are 65:22:13, surplus is Al and inevitable impurity.
Above-mentioned aluminum gallium alloy, is made up of the component of following mass percent：Ga 3.25~9.75%, In 1.1~
3.3%, Sn 0.65~1.95%, surplus is Al and inevitable impurity；Ga, In, Sn quality in the aluminum gallium alloy
Percentage sum is 5~15%, and described Ga, In, Sn mass ratio are 65:22:13.
Ga, In, Sn mass percent sum are preferably 8~12% in the aluminum gallium alloy.
The preparation method of above-mentioned aluminum gallium alloy, comprises the following steps：
By raw material A l, Ga, In, Sn vacuum be 1.8 × 10-4Pa~2.2 × 10-4Under conditions of Pa, argon gas is filled with extremely
Air pressure is 0.25atm~0.35atm in vacuum drying oven, and using 400~600A electric current molten alloy, cooling is produced.
Above-mentioned raw materials Al, Ga, In, Sn carry out melting in the water jacketed copper crucible of vacuum drying oven, cool down afterwards.
A kind of preparation method of aluminium hydrate nano rod, above-mentioned aluminum gallium alloy and water is reacted, after reaction terminates, by upper strata
Suspension is disperseed after 3-5min using ultrasonic wave, is evaporated moisture, is produced aluminium hydrate nano rod.
When above-mentioned aluminum gallium alloy reacts with water, every 3~10g aluminum gallium alloys correspondence 100mL water.The water is pure water.
The aluminum gallium alloy is 30~1000s with the time that water reacts.
Above-mentioned reaction temperature is room temperature.Reacted at room temperature, reaction condition is gentle and the reaction time is short.
It is above-mentioned that upper strata suspension is scattered specifically using ultrasonic wave：After reaction terminates, upper strata suspension is taken out and is placed in
In beaker, then carry out ultrasonic wave and disperse.
The ultrasonic power that the ultrasonic wave is disperseed is 200~350W.Disperseed using ultrasonic wave, make aluminium hydroxide
Molecule is constantly in motion state, plays good peptizaiton, can prevent the reunion of aluminum hydroxide particles, is conducive to preparing
Aluminium hydrate nano rod.
The Al-Ga-In-Sn alloys that low-melting-point metal (Ga, In, Sn) is obtained are added into aluminium, what Ga, In, Sn were formed
Low melting point phase (Ga-In-Sn eutectics, GIS) will be covered in aluminium grain surface, not only destroy the integrality of alumite, be also ginseng
Diffusion admittance is provided with the aluminium of reaction, can significantly promote aluminum-water reaction.Aluminum gallium alloy of the present invention occurs to swash at room temperature with water
Strong reaction, and be swift in response.
A kind of aluminium hydrate nano rod, is made using the preparation method of above-mentioned aluminium hydrate nano rod.
The granularity of the aluminium hydrate nano rod is 100nm~1 μm.The purity of the aluminium hydrate nano rod is reachable
More than 99.99%.
The beneficial effects of the invention are as follows：
Aluminum gallium alloy of the present invention, available for preparing aluminium hydrate nano rod, the low melting point phase (Ga- that Ga, In, Sn are formed
In-Sn eutectics, GIS) aluminium grain surface is covered in, the integrality of alumite is not only destroyed, is also provided to participate in the aluminium of reaction
Diffusion admittance, can significantly promote aluminum-water reaction.
The preparation method of aluminum gallium alloy of the present invention, aluminum gallium alloy is prepared using vacuum arc melting technology, and vacuum arc melts
Refining is cooled down using water jacketed copper crucible, compared to other melting techniques, and vacuum arc melting technology cooling velocity is exceedingly fast, and is
Rapid solidification, cooling velocity has important influence to crystallization in liquid phase process of setting, even if the alloy of identical component is in difference
Entirely different microstructure can be obtained under cooldown rate.
Unbiased in the Al-Ga-In-Sn alloys that the present invention is prepared using vacuum arc melting technology, its process of setting
Analysis or few segregation, and alloy structure is more uniform, Ga-In-Sn mass ratio and each component ratio phase in GIS ternary eutectics in alloy
Together.
The aluminum gallium alloy that the present invention is obtained using vacuum arc melting technology prepares aluminium hydrate nano rod, utilizes vacuum electric
Al-Ga-In-Sn alloys prepared by arc melting technique carry out reaction with water can obtain the higher aluminium hydrate nano rod of purity,
Realize that nano-aluminum hydroxide pattern is adjustable, grain size is adjustable.Because the fusing point of GIS ternary eutectics is minimum, and gallium aluminium of the present invention
Ga-In-Sn mass ratio is identical with mass ratio of each component example in GIS ternary eutectics in alloy, so the GIS phases that the present invention is formed
Composition is close to GIS ternary eutectic compositions, therefore GIS phases fusing point of the present invention is minimum.The reaction of Al-Ga-In-Sn alloys and water it is main according to
By the GIS phases of low melting point, so under the aluminum gallium alloy composition of the present invention, aluminum gallium alloy can quickly be carried out instead in room temperature with water
Should, the reaction time is in 30~1000s.
Under the aluminum gallium alloy member condition of the present invention, alloy aluminum water reaction rate is significantly improved, and the aluminium more than 90% exists
Aluminium hydrate nano rod is converted into very short time, production efficiency is greatly improved.The preparation side of aluminium hydrate nano rod of the present invention
Method, alloy is directly reacted with water, and technical process is simple, production efficiency is high, preparation condition is gentle, cost is relatively low and to environment
It is pollution-free.
Aluminium hydrate nano rod size produced by the present invention is small, and granularity is about 100nm~1 μm, and purity is up to 99.99%
More than.
Brief description of the drawings
Fig. 1 is the SEM figures that the gained aluminium hydrate nano rod of embodiment 1 amplifies 20000 times；
Fig. 2 is the SEM figures that the gained aluminium hydrate nano rod of embodiment 1 amplifies 40000 times；
Fig. 3 is the SEM figures that the gained aluminium hydrate nano rod of embodiment 2 amplifies 20000 times；
Fig. 4 is the SEM figures that the gained aluminium hydrate nano rod of embodiment 2 amplifies 40000 times；
Fig. 5 is the XRD of the gained aluminium hydrate nano rod of embodiment 2；
Fig. 6 is the EDS energy spectrum diagrams of the gained aluminium hydrate nano rod of embodiment 2.
Embodiment
Embodiment 1
The present embodiment aluminum gallium alloy, is made up of the component of following mass percent：Ga 3.25%, In 1.1%, Sn
0.65%, surplus is Al and inevitable impurity；Ga, In, Sn mass percent sum are 5% in aluminum gallium alloy, described
Ga, In, Sn mass ratio are 65:22:13.
The preparation method of the present embodiment aluminum gallium alloy, comprises the following steps：
1) raw material A l, Ga, In, Sn are weighed by composition proportion, are sequentially placed into the water jacketed copper crucible of vacuum drying oven；2) will be true
Empty stove back end is evacuated to 1.8 × 10-4Under the conditions of Pa, it is 0.25atm to be filled with air pressure in high-purity argon gas to vacuum drying oven, using 400A
Electric current molten alloy, cooling, produce, in fusion process, using electromagnetic force stir liquid alloy, ingot overturning melting 3 times,
To ensure that alloying component is tried one's best uniformly.
The preparation method of the present embodiment aluminium hydrate nano rod, comprises the following steps：
Take above-mentioned gained aluminum gallium alloy 3g and 100mL water to be reacted, react at room temperature 1000s, treat that aluminum gallium alloy is anti-with water
After answering completely, the suspension on reaction vessel upper strata is placed in beaker, then it disperseed using ultrasonic wave, ultrasonic power
For 200W, ultrasonic time is 3min, obtained aluminum hydroxide suspension will be then reacted as in beaker, by moisture in room temperature bar
It is evaporated naturally under part, you can obtain the aluminium hydrate nano rod that particle mean size is about 350nm, as shown in figure 1, being 20000 amplifications
The aluminium hydrate nano rod SEM figures of multiple；It is illustrated in figure 2 the aluminium hydrate nano rod SEM figures of 40000 multiplication factors.
Embodiment 2
The present embodiment aluminum gallium alloy, is made up of the component of following mass percent：Ga 9.75%, In 3.3%, Sn
1.95%, surplus is Al and inevitable impurity；Ga, In, Sn mass percent sum are 15% in aluminum gallium alloy, described
Ga, In, Sn mass ratio are 65:22:13.
The preparation method of the present embodiment aluminum gallium alloy, comprises the following steps：
1) raw material A l, Ga, In, Sn are weighed by composition proportion, are sequentially placed into the water jacketed copper crucible of vacuum drying oven；2) will be true
Empty stove back end is evacuated to 2.0 × 10-4Under the conditions of Pa, it is 0.3atm to be filled with air pressure in high-purity argon gas to vacuum drying oven, using 500A
Electric current molten alloy, cooling, produce, in fusion process, using electromagnetic force stir liquid alloy, ingot overturning melting 3 times,
To ensure that alloying component is tried one's best uniformly.
The preparation method of the present embodiment aluminium hydrate nano rod, comprises the following steps：
Take above-mentioned gained aluminum gallium alloy 3g and 100mL water to be reacted, react at room temperature 30s, treat that aluminum gallium alloy reacts with water
After completely, the suspension on reaction vessel upper strata is placed in beaker, then it disperseed using ultrasonic wave, ultrasonic power is
300W, ultrasonic time is 5min, will then react obtained aluminum hydroxide suspension as in beaker by moisture in room temperature condition
It is lower to be evaporated naturally, you can to obtain the aluminium hydrate nano rod that particle mean size is about 150nm, as shown in figure 3, being 20000 times of amplifications
The aluminium hydrate nano rod SEM figures of multiple；It is illustrated in figure 4 the aluminium hydrate nano rod SEM figures of 40000 times of multiplication factors.
Embodiment 3
The present embodiment aluminum gallium alloy, is made up of the component of following mass percent：Ga 7.8%, In 2.64%, Sn
1.56%, surplus is Al and inevitable impurity；Ga, In, Sn mass percent sum are 12% in aluminum gallium alloy, described
Ga, In, Sn mass ratio are 65:22:13.
The preparation method of the present embodiment aluminum gallium alloy, comprises the following steps：
1) raw material A l, Ga, In, Sn are weighed by composition proportion, are sequentially placed into the water jacketed copper crucible of vacuum drying oven；2) will be true
Empty stove back end is evacuated to 2.2 × 10-4Under the conditions of Pa, it is 0.35atm to be filled with air pressure in high-purity argon gas to vacuum drying oven, using 550A
Electric current molten alloy, cooling, produce, in fusion process, using electromagnetic force stir liquid alloy, ingot overturning melting 3 times,
To ensure that alloying component is tried one's best uniformly.
The preparation method of the present embodiment aluminium hydrate nano rod, comprises the following steps：
Take above-mentioned gained aluminum gallium alloy 10g and 100mL water to be reacted, react at room temperature 100s, treat that aluminum gallium alloy is anti-with water
After answering completely, the suspension on reaction vessel upper strata is placed in beaker, then it disperseed using ultrasonic wave, ultrasonic power
For 300W, ultrasonic time is 4min, will then react obtained aluminum hydroxide suspension as in beaker by moisture in room temperature bar
It is evaporated naturally under part, produces aluminium hydrate nano rod.
Embodiment 4
The present embodiment aluminum gallium alloy, is made up of the component of following mass percent：Ga 5.2%, In 1.76%, Sn
1.04%, surplus is Al and inevitable impurity；Ga, In, Sn mass percent sum are 8% in the aluminum gallium alloy,
Described Ga, In, Sn mass ratio are 65:22:13.
The preparation method of the present embodiment aluminum gallium alloy, comprises the following steps：
1) raw material A l, Ga, In, Sn are weighed by composition proportion, are sequentially placed into the water jacketed copper crucible of vacuum drying oven；2) will be true
Empty stove back end is evacuated to 2.0 × 10-4Under the conditions of Pa, it is 0.3atm to be filled with air pressure in high-purity argon gas to vacuum drying oven, using 600A
Electric current molten alloy, cooling, produce, in fusion process, using electromagnetic force stir liquid alloy, ingot overturning melting 3 times,
To ensure that alloying component is tried one's best uniformly.
The preparation method of the present embodiment aluminium hydrate nano rod, comprises the following steps：
Take above-mentioned gained aluminum gallium alloy 8g and 100mL water to be reacted, react at room temperature 500s, treat that aluminum gallium alloy reacts with water
After completely, the suspension on reaction vessel upper strata is placed in beaker, then it disperseed using ultrasonic wave, ultrasonic power is
350W, ultrasonic time is 4min, will then react obtained aluminum hydroxide suspension as in beaker by moisture in room temperature condition
It is lower to be evaporated naturally, produce aluminium hydrate nano rod.
Experimental example 1
XRD tests are carried out to the gained aluminium hydrate nano rod of embodiment 2, as a result as shown in figure 5, from Fig. 5, gained
Aluminium hydrate nano rod purity is high.
Experimental example 2
EDS tests are carried out to the gained aluminium hydrate nano rod of embodiment 2, as shown in fig. 6, the EDS of the a-quadrant in Fig. 6 (a)
Shown in collection of illustrative plates such as Fig. 6 (b), test data is as shown in table 1.From table 1 it follows that Al and O atomic ratio is 1：3.5, connect
Nearly Al (OH)3Middle Al and O atomic ratio 1：3, in conjunction with the XRD results in experimental example 1, it can be well demonstrated that products therefrom is
Al(OH)3。
The gained aluminium hydrate nano rod EDS data of 1 embodiment of table 2
Claims (8)
1. a kind of aluminum gallium alloy, it is characterised in that in the aluminum gallium alloy Ga, In, Sn mass percent sum be 5~
15%, described Ga, In, Sn mass ratio are 65:22:13, surplus is Al and inevitable impurity.
2. a kind of preparation method of aluminum gallium alloy as claimed in claim 1, it is characterised in that comprise the following steps：By raw material
Al, Ga, In, Sn are 1.8 × 10 in vacuum-4Pa~2.2 × 10-4Under conditions of Pa, being filled with air pressure in argon gas to vacuum drying oven is
0.25atm~0.35atm, using 400A~600A electric current molten alloy, cooling is produced.
3. a kind of preparation method of aluminium hydrate nano rod, it is characterised in that comprise the following steps：Will be as claimed in claim 1
Aluminum gallium alloy and water react, after reaction terminates, upper strata suspension is disperseed after 3-5min using ultrasonic wave, moisture is evaporated, i.e.,
Obtain aluminium hydrate nano rod.
4. the preparation method of aluminium hydrate nano rod as claimed in claim 3, it is characterised in that the aluminum gallium alloy and water are anti-
At once, every 3~10g aluminum gallium alloys correspondence 100mL water.
5. the preparation method of aluminium hydrate nano rod as claimed in claim 3, it is characterised in that the aluminum gallium alloy and water are anti-
The time answered is 30~1000s.
6. the preparation method of aluminium hydrate nano rod as claimed in claim 3, it is characterised in that the ultrasonic wave is scattered to be surpassed
Acoustical power is 200~350W.
7. a kind of aluminium hydrate nano rod, it is characterised in that be made using preparation method as claimed in claim 3.
8. aluminium hydrate nano rod as claimed in claim 7, it is characterised in that the granularity of the aluminium hydrate nano rod is
100nm~1 μm.
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| CN109399678A (en) * | 2018-11-14 | 2019-03-01 | 大连理工大学 | A kind of preparation method of nano level metal hydroxide |
| CN112110463A (en) * | 2019-06-19 | 2020-12-22 | 吉林大学 | Al (OH) based on aluminum-gallium-based alloy3Powder preparation method |
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| CN109399678B (en) * | 2018-11-14 | 2020-07-14 | 大连理工大学 | Preparation method of nano-scale metal hydroxide |
| CN112110463A (en) * | 2019-06-19 | 2020-12-22 | 吉林大学 | Al (OH) based on aluminum-gallium-based alloy3Powder preparation method |
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